Viscose spinning solution



Patented May 9, 1944 UNITED STATES PATENT O F viscosn $1 1 133; SOLUTION I Q l to North American Rayon Corporation, New York, N. Y., a corporation of Delaware No Drawing.

Original application January 29,

1940, Serial No. 316,277. Divided and this application August 28, 1942, Serial No. 456,557

4 Claims.

. cose solution is continuously extruded through the minute orifices of a spinneret into a coagulating or setting bath. However, since the introduction of the viscose process great troubles have been and are still experienced as far as continuous spinning is concerned due to impuri- I vidual filaments start to tear and occasion interruption of the spinning process.

Cation-active compounds are surface-active compounds which carry in the cation a hydrocarbon chain having 8 or more carbon atoms. They are particularly advantageous because they may be used in neutral salt, alkaline and acidic aqueous solutions, and also in hard water. In contradistinction to cation-active compounds, anion-active compounds are surface-active compounds which carry in the anion a more or less extended hydrocarbon chain. They flocculate in neutral salt, alkaline and acidic aqueous solutions, and also in hard water. Common soaps, etc., are anion-active compounds, and due to their instability in acid spin baths they are unable to prevent the incrustation of spinnerets and spinneret orifices. I

Incrustation inhibitors, in accordance with the present invention, may be prepared from sulphides derived from monosaccharides of the ketose or aldose type containing 5 or 6 carbon atoms. These sugar sulphides may be prepared from glucose, galactose, fructose, xylose, arabicnose, mannose, rhamnose, ribose, talose,-etc.

I have found that the contamination of spinnerets and clogging of spinneret orifices may be substantially overcome by spinningviscose solutions in the presence of cation-active monosaccharide derivatives having the general structure:

in which n is 5 or 6, R1 is a higher aliphatic radical having 8 or more carbon atoms, R2 represents an aliphaticor aromatic radical, and Ac reprecents an innocuous anion, such as an OH group or a negative acid radical. R2 may also represent the radical in this structure 01. (OH) n-lHm- These inhibitors may be prepared by reacting plain or mixed sulphides of monosaccharides with alkyl, aralkyl or aryl halides in conventional manner in accordance with the following equation:

Although these cation-active incrustation inhibitors may form corresponding bases in viscose solutions and salts in acid spin baths, they retain their surface-activity and, thus their property of substantially preventing incrustations on prolonged spinning. these cation-active compounds are added to viscose solutions or spin baths the physical characteristics such as strength, plasticity, lustre, etc., of regenerated'cellulose produced therefrom or therein, respectively, remain unaltered. Upon increasing the amount of incrustation inhibitor in a given viscose solution or spin bath, the regenerated cellulose produced therefrom or therein, respectively, may alter its physical characteristics, i. e., it may acquire a soft-lustre, become more plastic, lose part of its original strength, etc. For such reasons, the amounts to be added to viscose solutions or spin baths must be predetermined by experimentation. Additions of about 0.3 to 5.0 grams per liter of viscose solution are generally sufiicient to allow continuous spinning Without substantially afiecting the inherent physical characteristics of regenerated cellulose threads or films. Although these cation-active incrustation inhibitors improve the spinning of any conventional viscose solution or spin bath, I have found that they are especially .ever, this prior art does not disclose the prevention of incrustations by means of cation-active compounds.

Examples of suitable incrustation inhibitors are: methyl-fructyl-octyl sulphonium chloride, ethyl-fructyl-octyl sulphonium chloride, methyl- If very small amounts of glucyl-octyl sulphonium bromide, ,methyl-glucyldodecyl sulphonium bromide, methyl-glucyl-dodecyl sulphonium hydroxide, ethyl-glucyl-doa de'cyl sulphonium sulphate, methyl-glycyl-cetyl sulphonium bromide, phenyl-glucyl-dodecyl sulphonium bromide, bemtyl-glucyL-dodecyl.broemide, propyl glucyl-octyl sulphonium iodide; methyl galactyl octyl sulphonium bromide, ethyl galactyloctyl sulphonium methyl sulphate, etc. However, I wish to emphasize that the present invention is not limited to the com pounds enumerated above, since any cation active compound having the structure'set forth" above may be used provided it is suiiiciently 'sol-" uble and stable in viscose solutions and/or acid cal-having at least 8 carbon atoms. R2 represents in .is a number selected from the group consisting of 5 and 6, Bi is a higher aliphatic radia radical selected from the group consisting of sents asiibstitueiit selected iro'm' the group con- :sistinggj'oi i OH and negative jacid radicals, said derivative being-present in= said viscose solution in an amountsufllcient to substantially inhibit ihcrustation "of; spinnerets.

2. .A viscose-spinning solution containing a dis- 1 'so1ve'd;"s'ubstantially stable, cationeactive monospin baths to furnish surface-active cations;

therein.

Example I About 0.1 to 5 grams of methyl-glucyl-dodecyl' sulphonium bromide is added to one liter oifa conventional acid spin bath. When a viscose solution is extruded therein through the fine orifices of a corrosion-resistant spinneret (for example a platinum alloy spinneret) the incrustation of the spinneret orifices is substantially inhibited.

Example II Viscose filaments are spun in the presence of a small amount of ethyl-glucyl-dodecyl sulphonium bromide with the result that the spinneret orifices remain clean for long periods of time.

Example III About 0.1,to 5 grams of methyl-glucyl-dodecyl sulphoniurn bromide is added to one liter of -a conventional viscose spinning solution. When this solutionis extruded into an acid spin bath to form filaments therein the spinneretsfsub merged in the spin bath, remain substantially free from incrustations.

Example IV I The cation-active monosaccharide derivatives are added in small amounts to both the viscose solution and the acid spin bath in order to substantially prevent incrustation of spinneret orifices through which the viscose solution is extruded into the spin bath to form regenerated cellulose.

Modifications of my invention will readily be recognized by those skilled in the art, and I desire to include all modifications and variations coming within the scope of the appended claims.

This is a division of my application Serial No. 316,277, filed January 29, 1940, now Patent Number 2,294,378, issued September 1, 1942, which inturn is va continuation in part of my application Serial No. 233,826, filed October 'I, 1938.

I claim:

1. A viscose spinning solution containing a dissolved, substantially stable, cation-activemonosaccharide derivative having the structure:

Iii

sa'ccharidederivative having the structure:

in whichn is a number selected from the group consisting of {rand 6, R1 is a higher aliphatic radical having at least 8 carbonatomsrlhrep- "resentsan'alkyl radical, and Ac represents a substituent selected from the group consisting of OH and negative acid radicals, said derivativev being present in said viscose solution in an amount sufficient to substantially inhibit incrustation of spinnerets.

3. A viscose spinning solution containing a dissolved, substantially stable, cation-active mono- '-saccharide derivative having the structure:

in whicnn is a number selected from the group consisting of 5 and 6, R1 is a higher aliphatic radical having at least 8 carbon atoms, R: represents an aryl radical, and Ac represents a substituent selected from the group consisting of OH and negative acid radicals, said derivative being present in said viscose solution in an amount sufficient to substantially inhibit incrustation of spinnerets.

RUDOLPH S. BLEY. 

